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p-Toluenesulfonic acid → HCID 59354801, 화합물

HRID 1776357
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반응식

HRID 1776357 반응식
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:8]([C:11](=[O:22])[C:12]#[C:13][C:14]([CH3:21])([O:16][Si](C)(C)C)[CH3:15])=[CH:7][C:4]=1[C:5]#[N:6].CC1C=CC(S(O)(=O)=O)=CC=1>C(Cl)Cl.O>[OH:16][C:14]([CH3:21])([CH3:15])[C:13]#[C:12][C:11]([C:8]1[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[C:4]([CH:7]=1)[C:5]#[N:6])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 593548212-Methoxy-5-(4-methyl-4-(trimethylsilyloxy)pent-2-ynoyl)benzonitrile

생성물 1

HCID 59354801HCID 59354801, 화합물수율 122.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 2-methoxy-5-(4-methyl-4-(trimethylsilyloxy)pent-2-ynoyl)benzonitrile (1.2 g, 3.01 mmol) in DCM (20 mL) was added PTSA (1.08 g, 5.60 mmol) at RT. The reaction mixture was stirred for 30 minutes and diluted with water (5 mL). The combined organic layers were then washed with a saturated NaHCO3 solution and water, dried over Na2SO4, filtered, and then concentrated in vacuo to afford 5-(4-hydroxy-4-methylpent-2-ynoyl)-2-methoxybenzonitrile (0.9 g, 97%) as a semi-solid.

후처리

  1. washThe combined organic layers were then washed with a saturated NaHCO3 solution and water
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0f6451a8954047fdb7b8adb0027386ac
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09265767B2

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